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EP3234082B1 - Method for the extraction of oily components from coffee beans and/or of residual materials of coffee production - Google Patents

Method for the extraction of oily components from coffee beans and/or of residual materials of coffee production Download PDF

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Publication number
EP3234082B1
EP3234082B1 EP15816418.6A EP15816418A EP3234082B1 EP 3234082 B1 EP3234082 B1 EP 3234082B1 EP 15816418 A EP15816418 A EP 15816418A EP 3234082 B1 EP3234082 B1 EP 3234082B1
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EP
European Patent Office
Prior art keywords
coffee
extraction
oil
extracting agent
solvent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Not-in-force
Application number
EP15816418.6A
Other languages
German (de)
French (fr)
Other versions
EP3234082A1 (en
Inventor
Anja Glisovic
Stefan Handrick
Frank Hinrichs
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Gcr - Global Commodity Resources Ug (haftungsbeschrankt)
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Gcr - Global Commodity Resources Ug (haftungsbeschrankt)
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Publication of EP3234082A1 publication Critical patent/EP3234082A1/en
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Classifications

    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23FCOFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F5/00Coffee; Coffee substitutes; Preparations thereof
    • A23F5/46Coffee flavour; Coffee oil; Flavouring of coffee or coffee extract
    • A23F5/48Isolation or recuperation of coffee flavour or coffee oil
    • A23F5/483Isolation or recuperation of coffee flavour or coffee oil by solvent extraction of the beans, ground or not
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/12Refining fats or fatty oils by distillation

Definitions

  • the present invention relates to a process for the extraction of oily constituents from coffee beans and / or waste coffee production, which have a residual moisture content.
  • oil especially vegetable oil
  • the oil-containing material is first dried and ground (conditioned) and then subjected to one or two successive methods. Usually, in the latter case, it is first pressed and then extracted. If it is high oil content materials, such as Rapeseed, presses has the advantage that it is technically relatively simple and sufficiently efficient to be used in a cost-effective and profitable manner. By pressing, up to 90% of the oil can be extracted from one material. Disadvantages are squeezed in addition to the oil and suspended solids, which is why the oil has to go through several purification steps.
  • the extraction of oil is usually carried out by means of hexane.
  • the advantage of the extraction is the high efficiency and the purity of the oil. It can be recovered up to 98% of the oil, which is pure after the distillation of the extractant and normally requires no further treatment.
  • the extraction of oil from plant materials with hexane as a solvent is currently the established industry standard and has two key aspects that directly affect oil yield and hence the efficiency and economics of the process.
  • the first aspect is the solution efficiency, which describes how much oil per quantity of solvent and extraction material is accessible and can be dissolved in which time. This aspect is significantly influenced by the type of solvent, the composition of the oil, the working temperature, the conditioning of the oily material, the moisture content, and some other, less important factors.
  • the second aspect is the withdrawal of the solvent-oil mixture (Miscella) from the extraction material. Ideally, at the end of the extraction, the material will no longer contain any oil and only pure solvent, which will be recovered in a subsequent step.
  • the extraction is made possible by extraction systems, which can range from the small Soxhlet attachment in the laboratory to industrial countercurrent systems.
  • percolation plants are the most commonly used extractor for the extraction of oil.
  • a fluid flows through gravity through a porous one Material bed on a sieve bottom, a principle similar to the filtering of coffee.
  • the solvent usually hexane
  • the systems are operated at light underpressure and close to the boiling point of hexane at 69 ° C for reasons of fire safety, so that the temperature-dependent solution and diffusion process take place as quickly as possible.
  • the final step is to rinse with pure solvent that will cause the miscella with the lowest oil content to form during percolation through the material by taking up the least amount of oil. Subsequently, the extracted material is discharged and the extractant removed by steam distillation from the de-oiled extraction and recovered.
  • the so-called batch plants which are often found in laboratories and research facilities because of their low material throughput, such as. the SPX e & e Pilot Extraction Unit
  • the extraction material is placed in a well drained screen basket.
  • the solvent is applied from the top and can percolate through the material. Due to the structure, the miscella can be withdrawn continuously.
  • the extractor can also be flooded with solvent and withdrawn only after a certain residence time. In this version, separate rinses of the extraction material are used so that the rinsing effect of rinsing to rinse reduces the oil content of the miscella and of the extraction material.
  • the number of possible flushes depends directly on the number and volume of the tanks, which are available for storage, the solvent and the miscella with different oil content. Depending on the design, it is also possible to remove the solvent directly from the extraction material in the extraction vessel without discharging, in which hot steam is introduced. Batch plants belong to the so-called deep bed plants.
  • the extraction material is applied here with a relatively small bed depth of 0.3 to 1.2 m thickness on a sieve plate, so that the top applied extraction agent can percolate through the material bed.
  • the sieve bottom can be designed here as a conveyor belt and continue to move with the material or be designed as a groove. In this case, the extraction material is moved forward by screws or chain hoists. Below the sieve bottom is located in both versions a subdivided into sections collection container for the Miscella. The miscella is pumped from one section to the material of the following section and collected.
  • the number of sections depends on the execution and material and is usually between four and twelve, with seven to eight sections occurring most frequently.
  • the miscella with the highest oil content which is not used again for extraction, but for distillation and thus for oil extraction.
  • the last section which is below the material, which is treated with fresh / pure solvent and then discharged, there is the miscella with the lowest oil content.
  • the advantage of these systems is continuous operation. However, in comparison with batch systems, somewhat higher safety standards are necessary, since the removal of the solvent by steam distillation requires the removal of the hexane-containing, deoiled extraction material from the extractor.
  • the oil-containing material such as oilseeds, oil crops and oil sands
  • disadvantageous is a high water content in the oil extraction by means of hexane or other nonpolar solvent, such as gasoline or kerosene. If the water content is too high (> 10%), the water impedes the penetration of the hydrophobic solvent into the material and thus the solution of the oil.
  • the recoverable oil content can sink to a no longer cost-covering measure, the oil production is uneconomical.
  • the water content must be reduced accordingly by dry storage or active drying.
  • the active drying requires that considerable amounts of energy must be applied in order to dry the material to a suitable water content. This is always a relevant factor when the raw material has a high water content of more than 20% and tends by this water content for fermentation or fouling and thus unusable. This occurs especially with organic materials such as algae, freshly harvested oilseeds and oily waste materials of the food industry, such as for example, coffee reason, on.
  • a material contains e.g. 30 wt .-% oil in the dry mass and has a water content of 55 wt .-% in the raw state, the following proportions result in one ton of wet material: 550 kg of water, 315 kg of base material and 135 kg of oil.
  • 500 kg or half a ton of water would have to be evaporated. If this can not be achieved over long periods of storage, this must be done using energy, which can lead to considerable costs and can also have a negative impact on the quality of the oil due to oxidative stress.
  • DD 229 148 A1 describes a process which allows a sufficiently efficient oil extraction with up to 20% water content in the material. This is achieved by pretreatment of the extraction material with alcohol or alcohol mixtures, wherein the amount of added alcohol should be between 5 to 7% of the water content in the extraction material. After treatment with alcohol followed by a simple extraction with hexane or another alkane or an alkane mixture (gasoline, kerosene).
  • US 8273248 B1 describes a method specifically for the extraction of oil from algae, which contains consecutive extraction steps after a drying step. First, reduce the water content and add alcohol or a mixture of alcohols to the algae. Subsequently, hexane, another alkane or an alkane mixture is added. The individual parts are then mixed together and left to rest. During the suspension of the mixture, there is a phase separation of the alkane phase and the water-alcohol phase, which are separated. From the phases oil and proteins can be obtained. For efficient extraction, the process must be repeated several times. Also for the in the patent US 8273248 B1 process called for special extraction plants, which have facilities for phase separation. Although both processes can produce oil from wet materials, either energy-intensive drying steps, multiple extraction and separation steps, or special equipment are still required. All these are factors which are high Cause costs and make the oil production unprofitable.
  • the patent WO 2012/138382 A1 discloses a method for the extraction of polar lipids from algae by the use of various extractants and in particular solvents with excess alcohol.
  • no vegetable oils in terms of triglycerides (neutral lipids) and fatty acids are extracted from moist material, but polar lipids.
  • dewatering and drying steps are an integral part of the process shown, while in the present invention these are excluded or reduced to a minimum.
  • Patent DE 69623762 T2 describes a method for obtaining terpenes, such as cafestolester, diethanol esters and isocafestol esters, by treating the coffee grounds with phosphoric acid and then extracting the terpenes.
  • the disadvantage is that the coffee grounds must be dried before extraction. Extracted oil is called terpene soiling and should not be extracted from the coffee grounds.
  • US 2010/0287823 A1 discloses a method for obtaining biofuels from ground coffee.
  • the coffee is first treated with water and then treated to obtain the triglycerides with an organic solvent such as methanol, ethanol, hexane or mixtures of organic solvents.
  • an organic solvent such as methanol, ethanol, hexane or mixtures of organic solvents.
  • the water is separated from the ground coffee prior to extraction by, for example, freeze-drying or distillation.
  • the present invention has for its object to provide a simple, universally applicable, efficient, economical method for the extraction of oil-containing components from still moist coffee beans and / or moist residues of coffee production.
  • the object is achieved by a method for wet extraction of oily components from coffee beans and / or residues of coffee production, wherein the coffee beans and / or residues of the coffee production a residual moisture content of 10 to 95% by mass, particularly preferably from 30 to 85 Ma. %, very particularly preferably from 45 to 85% by mass, measured on the total mass of the coffee beans and / or residues of the Coffee production, extracted with an extractant mixture consisting of at least one polar and one nonpolar solvent and wherein the extractant mixture contains the at least one non-polar solvent in a proportion of 45 to 95% by volume, measured on the total volume of the extractant.
  • Extraction referred to in the context of the invention, the extraction of at least one substance from the extraction material coffee beans and / or residues of coffee production with a liquid extractant mixture.
  • Moist extraction refers to an extraction in which still moist extraction material, with a residual moisture content, is used.
  • oil-containing constituents encompass all substances which can be extracted with the extractant mixture according to the invention from the extraction material coffee beans and / or residues of the coffee production.
  • the oil-containing constituents are preferably fatty acid esters, in particular triglycerides and vegetable fats.
  • Coffee beans referred to in the context of the invention all types of coffee beans, both roasted and unroasted and mixtures of these.
  • the coffee beans may be pretreated, such as sorted or ground.
  • Ground, un-extracted / brewed coffee beans are also referred to as ground coffee.
  • Residues of coffee production include according to the invention all types of residues (including coffee residues), both waste and by-products from the coffee industry. These include, for example, coffee grounds, ground coffee, separator and decanter sludge and mixtures thereof. Residuals are, for example, in the industrial Löskaffee pellet as well as in private households or catering.
  • the industrial production of Löskaffee essentially comprises the following steps, wherein the technical execution may vary in details depending on the company:
  • the beans are roasted and ground into ground coffee.
  • the ground coffee is then repeatedly extracted (scalded) by hot water and optionally under pressure, so that a coffee extract (also known as coffee) and a coffee base (brewed ground coffee) are produced.
  • the coffee extract is then cleaned by decanters and separators of coffee grounds residues, remaining coffee grounds is referred to as separator and decanter sludge.
  • Coffee extract residues are removed by means of belt presses or other techniques from the coffee grounds and returned to production after being cleaned by means of decanters and separators.
  • Coffee grounds, separator and decanter sludge are considered as waste in industry and sent for thermal recycling.
  • they can be supplied to the inventive method due to their high water and oil content.
  • Coffee grounds according to the invention denotes the remnants of the coffee, in particular the coffee powder and / or ground coffee, after this has been subjected to a brewing process, for example. Coffee reason arises among other things with the drinking coffee preparation but also with the production of soluble coffee as a waste product.
  • mixtures of coffee beans and residues of coffee production can be used.
  • Residual moisture content according to the invention, the content of water, which is located in the coffee beans and / or the residues of coffee production.
  • Extractant mixture is a mixture of solvents that can be used to extract the oily components.
  • the oil-containing components at least partially dissolve in the extractant mixture.
  • the extracted oily components are dissolved and / or undissolved in the extractant mixture.
  • the extractant mixture consists of a polar and a nonpolar solvent. Solvents are classified according to their polarity (hydrophilicity). Polar and nonpolar in the context of the invention also refer to which solvent is the more polar or non-polar solvent when comparing two solvents. The Elutrope series provides information about this, for example.
  • the polar and nonpolar solvents are preferably immiscible with each other, but at least in the stated proportions by volume, miscible.
  • the polar solvent is miscible with the at least one oil-containing component to be extracted.
  • -Alkane is according to the invention saturated, acyclic hydrocarbons having the general formula C n H 2n + 2, wherein n is an integer.
  • the alkane can consist of both a linear carbon skeleton, as well as their isomers and branched carbon chains.
  • the polar solvent used is preferably an alcohol having a chain length of from 1 to 10 carbon atoms, more preferably from 1 to 6 carbon atoms, most preferably selected from methanol, ethanol, propanol, butanol and hexanol, more preferably 2-propanol.
  • the extractant mixture contains the nonpolar solvent from 45 to 95% by volume, more preferably from 55 to 85% by volume, most preferably from 55 to 75% by volume, even more preferably from 60% by volume, based on the total volume of extractant.
  • mixtures of at least one polar and one non-polar solvent are used, usually an alkane and an alcohol.
  • Suitable mixtures for the moist extraction shown here are mixtures with an alkane content of at least 50 wt .-%, preferably between 55 and 95 wt .-% and in particular between 55 wt% and 85 wt.%.
  • the extraction mixture preferably contains the at least one polar solvent in a proportion of 5 to 55% by volume, more preferably 15 to 45% by volume, very preferably 25 to 45% by volume, even more preferably 40% by volume. -%, measured on the total volume of the extractant.
  • the extraction mixture preferably contains further polar and / or non-polar solvents having a volume fraction of from 0.5 to 40% by volume, more preferably from 0.5 to 35% by volume, very particularly preferably from 0.5 to 19% by volume on the total volume of the extractant mixture.
  • the other polar and / or non-polar solvents are selected from the polar and non-polar solvents according to the invention.
  • binary, tertiary or higher mixtures of different alcohols such as methanol, ethanol, propanol and butanol, etc. can be used as the alcoholic phase and mixtures of pentane, hexane, heptane, gasoline or kerosene and the like as the alkane phase.
  • binary, tertiary or higher mixtures of different alcohols such as methanol, ethanol, propanol and butanol, etc.
  • binary, tertiary or higher mixtures of different alcohols such as methanol, ethanol, propanol and butanol, etc.
  • pentane, hexane, heptane, gasoline or kerosene and the like as the alkane phase.
  • mixtures based on acetone and toluene are possible.
  • the extractant mixture is preferably used at a temperature above the ambient temperature but below the boiling point of the lowest-boiling solvent or the lowest-boiling azeotrope of the extractant mixture.
  • An azeotrope is a mixture of at least two solvents whose vapor phase has the same composition as the liquid phase, whereby a distillative separation of the at least two solvents is not possible.
  • the efficiency of the extraction process increases as all chemical and physical processes with increasing temperature.
  • the maximum working temperature corresponds to this Boiling point of the most volatile component of the extraction solution, which may also be an azeotrope of various components.
  • the temperature is chosen only so high that the oil-containing components to be extracted are not negatively changed by the applied heat.
  • a warm extractant mixture having a temperature of from 35 to 69.degree. C., very particularly preferably from 50 to 65.degree. C., very particularly preferably from 58 to 63.degree.
  • the temperature is only slightly (0 to 6 ° C) below the boiling point of n-hexane (boiling point: 69 ° C).
  • the extraction rate is increased by the use of a warm extractant mixture, i. It can be removed with an extractant mixture with elevated temperature, a larger amount of oily ingredients than with the same volume of the same extractant mixture which has only ambient temperature.
  • coffee beans and / or residues of the coffee production are used with an average particle size of 0.001 to 10 mm, more preferably from 0.01 to 5 mm, most preferably from 0.01 to 2 mm.
  • the coffee beans and / or residues of coffee production to at least 30% by mass, measured on the total weight of the coffee beans and / or residues of coffee production, an average grain size of less than or equal to 2 mm.
  • Grain size in the context of the invention means the average size distribution of the particles within a batch of coffee beans and / or residues of coffee production.
  • miscella refers to a mixture of an extraction (mixture) and at least one extracted oil.
  • the oil-bearing material may also be previously ground to obtain an optimum material size.
  • the maximum particle size should be less than 5 mm and better still less than 2 mm.
  • particle sizes below 1 mm are to be striven for, wherein at least 30% by weight of the oil-carrying material should have a particle size of less than 2 mm in the dry state.
  • Total dry mass denotes the total mass of the coffee beans and / or residues of the coffee production after its complete drying to constant mass.
  • 50 to 100% by mass, more preferably 65 to 99% by mass, most preferably 70 to 99% by mass of the oil-containing constituents, measured on the total mass of the coffee beans and / or the residues of the coffee production can be extracted.
  • the oil-containing components are separated by distillation after extraction from the extractant mixture.
  • the separation of the extracted oil-containing constituents from the extractant mixture can be carried out, for example, over several stages, wherein first the most volatile component and then successively the less volatile constituents are separated off.
  • an extractant mixture can be prepared from recovered solvent again. Distillation of the miscella separates the oil from the solvent, as in a conventional extraction process based on hexane as extractant.
  • the distillation not only the oil is separated from the extraction solution, but it can also be the components of the extractant separated from each other. If these are collected in the same container and combined, the mixture can be used again as an extractant. If the individual components are separated, the extractant can be adapted to different properties of the material to be extracted during operation if the structure of the system permits this. Due to the different constituents of the extractant, the individual components have a different tendency to remain in the de-oiled base material. As a result, the proportionate composition of the extraction solution changes over time and the ratio of the components leaves the preset optimal range. Accordingly, it is necessary to regularly check the composition of the extraction mixture and readjust if necessary.
  • mixtures of 50% by weight to 95% by weight of n-hexane and 5% by weight to 50% by weight of 2-propanol are used for extracting oily constituents from coffee beans and / or residues of coffee production used to dry without 70 - 98 wt .-% of the oil from materials (coffee beans and / or residues of coffee production) having a moisture content of 55 to 75 wt .-% and an oil content between 15 and 35 wt .-% in dry matter to win.
  • the oil is also miscible with the alcoholic phase and, ideally, also soluble in it. If this is the case, it is possible to dissolve more than 90% of the oil from moist, oily material and to separate it from the extractant by means of distillation, as in a conventional extraction process with n-hexane as solvent.
  • the process of moist extraction can be run on all systems which are designed for hexane extraction, such as percolation and continuous belt systems. Only the distillation unit must be able to operate at higher temperatures than when using pure hexane, since the alcohols usually have higher boiling points than hexane. If necessary, seals must be used which are able to withstand both alkanes and alcohols.
  • colorants and suspended matter can be converted into the extract from the material, which normally can not be found in the oil in a pure hexane extraction. This is due to the alcohol content, which allows the transfer of hydrophilic substances to some extent.
  • another filter step can be integrated into the process, which allows to remove any suspended solids from the oil. The further treatment of the oil takes place after the separation of the solvent and the filtration in an oil refiner and is no longer part of this process. Also can be optimized by a reduction of the alcohol content of the process to a purer oil out, if thereby the extraction efficiency is not or only reasonably suffers.
  • centrifuges or presses may be connected downstream in order to separate remaining extraction solution from the deoiled raw material.
  • current and initial investment costs are significantly reduced by the process according to the invention compared with the previously mentioned conventional and non-conventional extraction processes.
  • the process of the invention thus provides a simple and universally applicable, efficient, economical process for the extraction of vegetable oils based on triglycerides from still moist materials, such as coffee beans and / or coffee production residues.
  • the inventive method on all conventional extraction systems, if necessary with minimal modifications.
  • the coffee beans and / or remains of the coffee production are extracted several times with fresh extractant mixture.
  • the extraction is carried out one to 10 times, more preferably one to 7 times, most preferably one to 5 times, even more preferably three times.
  • the degree of extraction is thus increased, ie more oily constituent is obtained from the coffee beans and / or residues of the coffee production.
  • the individual extractant mixtures which are obtained after a multiple extraction of the coffee beans and / or remnants of the coffee production with each fresh extractant mixture, are advantageously combined. From the combined extractant mixtures, the oily components are removed by distillation.
  • the present method essentially deals with a method for increasing the solution efficiency of the extraction of moist materials, which for the first time enables the efficient and cost-efficient extraction of moist materials without prior drying.
  • the coffee grounds were also dried to determine the respective mass of the sample and thus to determine the maximum possible amount of oil to be extracted. This theoretical amount of oil and the amount of oil actually recovered were then put into proportion.
  • wet extraction it was possible to obtain between 50 and 95% by mass of the oil, the yield being between 90 and 97% with an n-hexane content of 70 and 85% by volume. Beyond this optimum range, extraction efficiency dropped rapidly and was at 0% yield for pure n-hexane (100% by volume).

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  • Engineering & Computer Science (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Wood Science & Technology (AREA)
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Description

Die vorliegende Erfindung betrifft ein Verfahren zur Extraktion von ölhaltigen Bestandteilen aus Kaffeebohnen und/oder Reststoffen der Kaffeeproduktion, die einen Restfeuchtegehalt aufweisen.The present invention relates to a process for the extraction of oily constituents from coffee beans and / or waste coffee production, which have a residual moisture content.

Der gegenwärtige Stand der Technik ist, dass Öl, insbesondere Pflanzenöl, entweder mittels Pressen oder Extraktion gewonnen wird. Zu diesem Zweck wird das ölhaltige Material zuerst getrocknet und gemahlen (konditioniert) und anschließend einer oder nacheinander beiden Methoden unterworfen. Üblicherweise wird im letzteren Fall zuerst gepresst und anschließend extrahiert. Wenn es sich um Materialien mit hohem Ölgehalt handelt, wie z.B. Rapssaat, hat Pressen den Vorteil, dass es technisch relativ einfach und hinreichend effizient ist, um kostendeckend und gewinnbringend eingesetzt zu werden. Durch Pressen können bis zu 90 % des Öls aus einem Material gewonnen werden. Nachteilig werden neben dem Öl auch Schwebstoffe ausgepresst, weshalb das Öl noch mehrere Reinigungsschritte durchlaufen muss.The current state of the art is that oil, especially vegetable oil, is recovered either by pressing or extraction. For this purpose, the oil-containing material is first dried and ground (conditioned) and then subjected to one or two successive methods. Usually, in the latter case, it is first pressed and then extracted. If it is high oil content materials, such as Rapeseed, presses has the advantage that it is technically relatively simple and sufficiently efficient to be used in a cost-effective and profitable manner. By pressing, up to 90% of the oil can be extracted from one material. Disadvantages are squeezed in addition to the oil and suspended solids, which is why the oil has to go through several purification steps.

Die Extraktion von Öl erfolgt üblicherweise mittels Hexan. Der Vorteil der Extraktion sind der hohe Wirkungsgrad und die Reinheit des Öls. Es können bis zu 98 % des Öls gewonnen werden, welches nach der Destillation des Extraktionsmittels rein vorliegt und normalerweise keiner weiteren Behandlung bedarf. Die Extraktion von Öl aus Pflanzenmaterialien mit Hexan als Lösungsmittel ist gegenwärtig der etablierte, industrielle Standard und hat zwei wesentliche Aspekte, welche die Ölausbeute direkt beeinflussen und damit die Effizienz und Wirtschaftlichkeit des Verfahrens. Der erste Aspekt ist die Lösungseffizienz, diese beschreibt wie viel Öl pro Menge Lösungsmittel und Extraktionsgut in welcher Zeit zugänglich ist und gelöst werden kann. Dieser Aspekt wird maßgeblich von der Art des Lösungsmittels, der Zusammensetzung des Öls, der Arbeitstemperatur, der Konditionierung des ölhaltigen Materials, dem Feuchtigkeitsgehalt und einigen weiteren, weniger wichtigen Faktoren beeinflusst. Der zweite Aspekt ist die Entzugsvollständigkeit des Lösungsmittel-Öl-Gemisches (Miscella) aus dem Extraktionsgut. Im Idealfall enthält das Material am Ende der Extraktion kein Öl mehr und nur noch reines Lösungsmittel, das in einem anschließenden Schritt wieder zurückgewonnen wird.The extraction of oil is usually carried out by means of hexane. The advantage of the extraction is the high efficiency and the purity of the oil. It can be recovered up to 98% of the oil, which is pure after the distillation of the extractant and normally requires no further treatment. The extraction of oil from plant materials with hexane as a solvent is currently the established industry standard and has two key aspects that directly affect oil yield and hence the efficiency and economics of the process. The first aspect is the solution efficiency, which describes how much oil per quantity of solvent and extraction material is accessible and can be dissolved in which time. This aspect is significantly influenced by the type of solvent, the composition of the oil, the working temperature, the conditioning of the oily material, the moisture content, and some other, less important factors. The second aspect is the withdrawal of the solvent-oil mixture (Miscella) from the extraction material. Ideally, at the end of the extraction, the material will no longer contain any oil and only pure solvent, which will be recovered in a subsequent step.

Technisch ermöglicht wird die Extraktion durch Extraktionsanlagen, die vom kleinen Soxhlet-Aufsatz im Labor bis zu industriellen Gegenstromanlagen reichen können. Von diesen sind Perkolationsanlagen der am häufigsten verwendete Extraktortyp für die Extraktion von Öl. Bei der Perkolation fließt eine Flüssigkeit getrieben durch die Schwerkraft durch ein poröses Materialbett auf einen Siebboden, ein Prinzip ähnlich dem Filtern von Kaffee. Während das Lösungsmittel (üblicherweise Hexan) nach unten durch das Bett aus ölhaltigem Material läuft (sickert), wird das Öl im Lösungsmittel gelöst, die Miscella entsteht, welche unterhalb des Siebbodens aufgefangen wird. In der Regel werden die Anlagen aus Brandschutzgründen bei leichtem Unterdruck und nahe dem Siedepunkt von Hexan bei 69 °C betrieben, so dass die temperaturabhängigen Lösung- und Diffusionsprozesses schnellst möglich ablaufen. Bei geeigneter Wahl der Flockengröße, der Restfeuchtigkeit, des Extraktionsmittels und der Temperatur kann hier eine Lösungseffizienz von 98-99 % erreicht werden. Dieses Prinzip ist allen Perkolationsanlagen gemein, allerdings sind durch die Notwendigkeit eine hinreichende Entzugsvollständigkeit und einen gewissen Materialdurchsatz zu erreichen, verschiedene Varianten von Perkolationsextraktionsanlagen entstanden, welche sich nach Hersteller und Anwendung stark unterscheiden. Gemeinsam ist ihnen allen, dass die Miscella mit dem höchsten Ölanteil immer am Anfang des Prozesses auf das Extraktionsgut gegeben wird, wenn dessen Ölgehalt ebenfalls am höchsten ist. Sukzessive wird dann die Miscella mit einem niedrigeren Ölanteil genutzt, um den Ölgehalt des Extraktionsgutes Schritt für Schritt zu reduzieren. Im letzten Schritt wird mit reinem Lösungsmittel gespült, das während der Perkolation durch das Material durch die Aufnahme von geringsten Mengen Öl die Miscella mit dem niedrigsten Ölanteil entstehen lässt. Anschließend wird das extrahierte Material ausgeschleust und das Extraktionsmittel durch Dampfdestillation aus dem entölten Extraktionsgut entfernt und zurückgewonnen.Technically, the extraction is made possible by extraction systems, which can range from the small Soxhlet attachment in the laboratory to industrial countercurrent systems. Of these, percolation plants are the most commonly used extractor for the extraction of oil. In percolation, a fluid flows through gravity through a porous one Material bed on a sieve bottom, a principle similar to the filtering of coffee. As the solvent (usually hexane) passes down through the bed of oleaginous material, the oil is dissolved in the solvent to form the miscella, which is collected below the sieve tray. As a rule, the systems are operated at light underpressure and close to the boiling point of hexane at 69 ° C for reasons of fire safety, so that the temperature-dependent solution and diffusion process take place as quickly as possible. With a suitable choice of the flake size, the residual moisture, the extractant and the temperature, a solution efficiency of 98-99% can be achieved here. This principle is common to all percolation plants, but due to the need to achieve sufficient withdrawal completeness and a certain material throughput, different variants of percolation extraction plants have arisen, which differ greatly according to manufacturer and application. Common to all of them is that the miscella with the highest oil content is always added to the extraction material at the beginning of the process, when its oil content is also highest. Successively, the miscella with a lower oil content is used to reduce the oil content of the extraction material step by step. The final step is to rinse with pure solvent that will cause the miscella with the lowest oil content to form during percolation through the material by taking up the least amount of oil. Subsequently, the extracted material is discharged and the extractant removed by steam distillation from the de-oiled extraction and recovered.

In der einfachsten Form, den sogenannten Batchanlagen, welche wegen ihres geringen Materialdurchsatzes oft in Laboratorien und Forschungseinrichtungen zu finden sind, wie z.B. der SPX e&e Pilot-Extraktionsanlage, wird das Extraktionsgut in einen durchlässigen Siebkorb gegeben. Das Lösungsmittel wird von oben aufgebracht und kann durch das Material perkolieren. Durch den Aufbau kann die Miscella kontinuierlich abgezogen werden. Alternativ kann der Extraktor auch mit Lösungsmittel geflutet und erst nach einer gewissen Verweildauer abgezogen werden. In dieser Ausführung wird mit separaten Spülungen des Extraktionsgutes gearbeitet, so dass von Spülung zu Spülung der Ölgehalt der Miscella und des Extraktionsgutes reduziert wird. Die Anzahl der möglichen Spülungen hängt dabei direkt mit der Anzahl und dem Volumen der Tanks ab, welche zur Lagerung das Lösungsmittels und der Miscella mit unterschiedlichem Ölanteil zur Verfügung stehen. Je nach Ausführung ist es auch möglich, das Lösungsmittel ohne ausschleusen direkt im Extraktionskessel aus dem Extraktionsgut zu entfernen, in dem heißer Dampf eingeleitet wird. Batchanlagen gehören zu den sogenannten Tiefbettanlagen.In the simplest form, the so-called batch plants, which are often found in laboratories and research facilities because of their low material throughput, such as. the SPX e & e Pilot Extraction Unit, the extraction material is placed in a well drained screen basket. The solvent is applied from the top and can percolate through the material. Due to the structure, the miscella can be withdrawn continuously. Alternatively, the extractor can also be flooded with solvent and withdrawn only after a certain residence time. In this version, separate rinses of the extraction material are used so that the rinsing effect of rinsing to rinse reduces the oil content of the miscella and of the extraction material. The number of possible flushes depends directly on the number and volume of the tanks, which are available for storage, the solvent and the miscella with different oil content. Depending on the design, it is also possible to remove the solvent directly from the extraction material in the extraction vessel without discharging, in which hot steam is introduced. Batch plants belong to the so-called deep bed plants.

Von ihnen zu unterscheiden sind die sogenannten Flachbettanlagen, welche für einen kontinuierlichen Materialstrom ausgelegt sind und entsprechend in Großanlagen zum Einsatz kommen. Das Extraktionsgut wird hier mit einer relativ geringen Betttiefe von 0,3 bis 1,2 m Dicke auf einen Siebboden aufgebracht, so dass das von oben aufgebrachte Extraktionsmittel durch das Materialbett perkolieren kann. Der Siebboden kann hierbei als Förderband ausgelegt sein und sich mit dem Material weiter bewegen oder auch fest als Rinne ausgeführt sein. In diesem Falle wird das Extraktionsgut durch Schnecken oder Kettenzüge vorwärts bewegt. Unterhalb des Siebbodens befindet sich bei beiden Ausführungen ein in Sektionen unterteilter Auffangbehälter für die Miscella. Die Miscella wird jeweils von einer Sektion auf das Material der Folgesektion gepumpt und aufgefangen. Die Anzahl der Sektionen ist hierbei ausführungs- und materialabhängig und beträgt meist zwischen vier und zwölf, wobei sieben bis acht Sektionen am häufigsten vorkommen. In der ersten Sektion des Miscellatanks, über der das frische, gerade eingeschleuste Material liegt, befindet sich die Miscella mit dem höchsten Ölanteil, welche nicht wieder zur Extraktion eingesetzt wird, sondern zur Destillation und damit zur Ölgewinnung geht. In der letzten Sektion, welche sich unterhalb des Materials befindet, welches mit frischem/reinem Lösungsmittel behandelt und anschließend ausgeschleust wird, befindet sich die Miscella mit dem geringsten Ölanteil. Der Vorteil dieser Anlagen liegt im kontinuierlichen Betrieb. Allerdings sind im Vergleich zu Batchanlagen etwas höhere Sicherheitsstandards notwendig, da für den Entzug des Lösungsmittels durch Dampfdestillation das Hexan enthaltende, entölte Extraktionsgut aus dem Extraktor geschleust werden muss.To distinguish them from the so-called flat bed plants, which are designed for a continuous flow of material and are used accordingly in large plants come. The extraction material is applied here with a relatively small bed depth of 0.3 to 1.2 m thickness on a sieve plate, so that the top applied extraction agent can percolate through the material bed. The sieve bottom can be designed here as a conveyor belt and continue to move with the material or be designed as a groove. In this case, the extraction material is moved forward by screws or chain hoists. Below the sieve bottom is located in both versions a subdivided into sections collection container for the Miscella. The miscella is pumped from one section to the material of the following section and collected. The number of sections depends on the execution and material and is usually between four and twelve, with seven to eight sections occurring most frequently. In the first section of the Miscellatank, over which the fresh, just introduced material lies, is the miscella with the highest oil content, which is not used again for extraction, but for distillation and thus for oil extraction. In the last section, which is below the material, which is treated with fresh / pure solvent and then discharged, there is the miscella with the lowest oil content. The advantage of these systems is continuous operation. However, in comparison with batch systems, somewhat higher safety standards are necessary, since the removal of the solvent by steam distillation requires the removal of the hexane-containing, deoiled extraction material from the extractor.

Gemeinsam ist allen industriell relevanten Methoden, dass das Öl enthaltende Material, wie Ölsaaten, Ölfrüchte und Ölsande, einen Wassergehalt von weniger als 20 %, besser weniger als 10 % und bevorzugt um die 7 %, aufweisen sollte, um eine effiziente Gewinnung des Öls zu erlauben. Ist der Wasseranteil beim Pressen zu hoch, wird hauptsächlich Wasser und nur ein geringer Ölanteil aus dem Material gepresst. Ähnlich nachteilig wirkt sich ein hoher Wassergehalt bei der Ölextraktion mittels Hexan oder einem anderen unpolarem Lösungsmittel aus, wie z.B. Benzin oder Kerosin. Ist der Wasseranteil zu hoch (> 10 %), so behindert das Wasser das Eindringen des hydrophoben Lösungsmittels in das Material und damit die Lösung des Öls. Der gewinnbare Ölanteil kann so auf ein nicht mehr kostendeckendes Maß sinken, die Ölgewinnung wird unwirtschaftlich. Für eine wirtschaftlich interessante Ölgewinnung mittels der genannten Methoden muss der Wasseranteil entsprechend durch trockene Lagerung oder aktive Trocknung reduziert werden. Insbesondere die aktive Trocknung bedingt, dass erhebliche Energiemengen aufgebracht werden müssen, um das Material auf einen geeigneten Wassergehalt zu trocknen. Dies ist immer dann ein relevanter Faktor, wenn das Rohmaterial einen hohen Wasseranteil von mehr als 20 % besitzt und durch diesen Wassergehalt zur Fermentation oder Faulen neigt und dadurch unbrauchbar wird. Dies tritt besonders bei organischen Materialien, wie z.B. Algen, frisch geernteten Ölsaaten und ölhaltigen Abfallstoffen der Lebensmittelindustrie, wie beispielsweise Kaffeegrund, auf.Common to all industrially relevant methods is that the oil-containing material, such as oilseeds, oil crops and oil sands, should have a water content of less than 20%, better still less than 10%, and preferably around 7%, in order to efficiently recover the oil allow. If the water content during pressing is too high, mainly water and only a small proportion of oil is pressed out of the material. Similarly disadvantageous is a high water content in the oil extraction by means of hexane or other nonpolar solvent, such as gasoline or kerosene. If the water content is too high (> 10%), the water impedes the penetration of the hydrophobic solvent into the material and thus the solution of the oil. The recoverable oil content can sink to a no longer cost-covering measure, the oil production is uneconomical. For an economically interesting oil production by means of the mentioned methods, the water content must be reduced accordingly by dry storage or active drying. In particular, the active drying requires that considerable amounts of energy must be applied in order to dry the material to a suitable water content. This is always a relevant factor when the raw material has a high water content of more than 20% and tends by this water content for fermentation or fouling and thus unusable. This occurs especially with organic materials such as algae, freshly harvested oilseeds and oily waste materials of the food industry, such as for example, coffee reason, on.

Enthält ein Material z.B. 30 Gew.-% Öl in der Trockenmasse und hat im Rohzustand einen Wassergehalt von 55 Gew.-%, so ergeben sich folgende Anteile bei einer Tonne feuchtem Material: 550 kg Wasser, 315 kg Grundmaterial und 135 kg Öl. Um das Material auf einen Feuchtigkeitsgrad von 10 % zu bringen, müssten also 500 kg oder eine halbe Tonne Wasser verdampft werden. Kann dies nicht über lange Lagerzeiten erzielt werden, so muss dies unter Energieeinsatz erfolgen, was erhebliche Kosten verursacht und auch die Qualität des Öls durch oxidativen Stress negativ beeinflussen kann. Da die Verdampfungsenthalpie von Wasser bei 2,26 MJ/kg liegt, sind mindestens 1130 MJ (500 kg · 2,26 MJ/kg) nötig, um das Material zu trocknen, wofür mindestens 28,25 kg Erdgas mit einem Heizwert von 40 MJ/kg aufgewendet werden müssten, was einen erheblichen Aufwand und Verbrauch von Ressourcen bedeutet. Eine Möglichkeit, ohne vorherige Trocknung und ohne aufwendige Spezialanlagen Öl aus feuchten Rohmaterialien zu extrahieren, ist in Zeiten steigender Energiepreise und steigendem Umweltbewusstseins wünschenswert.If a material contains e.g. 30 wt .-% oil in the dry mass and has a water content of 55 wt .-% in the raw state, the following proportions result in one ton of wet material: 550 kg of water, 315 kg of base material and 135 kg of oil. In order to bring the material to a moisture level of 10%, 500 kg or half a ton of water would have to be evaporated. If this can not be achieved over long periods of storage, this must be done using energy, which can lead to considerable costs and can also have a negative impact on the quality of the oil due to oxidative stress. Since the enthalpy of vaporization of water is 2.26 MJ / kg, at least 1130 MJ (500 kg · 2.26 MJ / kg) is required to dry the material for which at least 28.25 kg of natural gas with a calorific value of 40 MJ / kg would have to be spent, which means a considerable effort and consumption of resources. One way of extracting oil from wet raw materials without prior drying and without costly special equipment is desirable in times of rising energy prices and increasing environmental awareness.

Aus den Patenten DD 229148 A1 von 1984 und US 8273248 B1 von 2012 sind Verfahren bekannt, mit welchen Öl aus Materialien mit höherem Feuchtigkeitsgrad gewonnen werden kann.From the patents DD 229148 A1 of 1984 and US 8273248 B1 of 2012 There are known methods by which oil can be obtained from materials having a higher degree of moisture.

DD 229 148 A1 beschreibt ein Verfahren, welches mit bis zu 20 % Wassergehalt im Material eine hinreichend effiziente Ölextraktion erlaubt. Dies wird durch eine Vorbehandlung des Extraktionsgutes mit Alkohol oder Alkoholmischungen erreicht, wobei die Menge des zugegebenen Alkohols zwischen 5 bis 7 % des Wasseranteils im Extraktionsgut betragen soll. Nach der Behandlung mit Alkohol folgt eine einfache Extraktion mit Hexan oder einem anderen Alkan oder einem Alkangemisch (Benzin, Kerosin). DD 229 148 A1 describes a process which allows a sufficiently efficient oil extraction with up to 20% water content in the material. This is achieved by pretreatment of the extraction material with alcohol or alcohol mixtures, wherein the amount of added alcohol should be between 5 to 7% of the water content in the extraction material. After treatment with alcohol followed by a simple extraction with hexane or another alkane or an alkane mixture (gasoline, kerosene).

US 8273248 B1 beschreibt ein Verfahren spezifisch für die Extraktion von Öl aus Algen, welches nach einem Trocknungsschritt konsekutive Extraktionsschritte enthält. Zuerst wird der Wassergehalt reduziert und Alkohol oder ein Alkoholgemisch zu den Algen gegeben. Anschließend wird Hexan, ein anderes Alkan oder ein Alkangemisch zugegeben. Die einzelnen Anteile werden dann miteinander vermengt und ruhen gelassen. Während des Ruhens der Mischung, kommt es zu einer Phasenseparation der Alkanphase und der Wasser-Alkohol-Phase, welche getrennt werden. Aus den Phasen können Öl und Proteine gewonnen werden. Für eine effiziente Gewinnung muss der Prozess mehrmals wiederholt werden. Auch sind für den im Patent US 8273248 B1 genannten Prozess spezielle Extraktionsanlagen nötig, welche über Anlagen zu Trennung der Phasen verfügen. Zwar können beide Verfahren aus feuchten Materialien Öl gewinnen, doch sind immer noch entweder energieaufwändige Trocknungsschritte, mehrfache Extraktions- und Separationsschritte oder spezielle Anlagen nötig. Alles dies sind Faktoren, welche hohe Kosten verursachen und die Ölgewinnung unprofitabel machen können. US 8273248 B1 describes a method specifically for the extraction of oil from algae, which contains consecutive extraction steps after a drying step. First, reduce the water content and add alcohol or a mixture of alcohols to the algae. Subsequently, hexane, another alkane or an alkane mixture is added. The individual parts are then mixed together and left to rest. During the suspension of the mixture, there is a phase separation of the alkane phase and the water-alcohol phase, which are separated. From the phases oil and proteins can be obtained. For efficient extraction, the process must be repeated several times. Also for the in the patent US 8273248 B1 process called for special extraction plants, which have facilities for phase separation. Although both processes can produce oil from wet materials, either energy-intensive drying steps, multiple extraction and separation steps, or special equipment are still required. All these are factors which are high Cause costs and make the oil production unprofitable.

Das Patent WO 2012/138382 A1 offenbart eine Methode zur Extraktion von polaren Lipiden aus Algen mittels des Einsatzes verschiedener Extraktionsmittel und insbesondere von Lösungsmitteln mit Alkoholüberschuss. Insbesondere werden keine Pflanzenöle im Sinne von Triglyceriden (neutrale Lipide) und Fettsäuren aus feuchtem Material extrahiert, sondern polare Lipide. Nachteilig sind Entwässerungs- und Trocknungsschritte, ein integraler Teil des dargestellten Prozesses, während diese in der vorliegenden Erfindung ausgeschlossen bzw. auf ein Minimum reduziert sind.The patent WO 2012/138382 A1 discloses a method for the extraction of polar lipids from algae by the use of various extractants and in particular solvents with excess alcohol. In particular, no vegetable oils in terms of triglycerides (neutral lipids) and fatty acids are extracted from moist material, but polar lipids. Disadvantageously, dewatering and drying steps are an integral part of the process shown, while in the present invention these are excluded or reduced to a minimum.

In der EP 0617119A2 wird eine Methode zur gleichzeitigen Extraktion von hydrophobe Triterpenoide wie Azadirachtin und Öl aus der trockenen Saat des Neembaumes beschrieben. Nachteilig werden lediglich trockene Materialien extrahiert und die offenbarten Extraktionslösungen besitzen alle einen Überschuss an Alkohol. Das dargestellte Verfahren ist nicht auf die Gewinnung des Öls sondern auf die Gewinnung von hydrophilen Bestandteilen optimiert.In the EP 0617119A2 describes a method for the simultaneous extraction of hydrophobic triterpenoids such as azadirachtin and oil from the dry seed of the neem tree. Disadvantageously, only dry materials are extracted and the disclosed extraction solutions all have an excess of alcohol. The illustrated method is not optimized for the recovery of the oil but for the recovery of hydrophilic components.

Patent DE 69623762 T2 beschreibt eine Methode zur Gewinnung von Terpenen, wie Cafestolester, Kahweolester und Isocafestolester durch eine Behandlung des Kaffeesatzes mit Phosphorsäure und anschließender Extraktion der Terpene. Nachteilig muss der Kaffeesatz vor der Extraktion getrocknet werden. Mit extrahiertes Öl wird als Verschmutzung der Terpene genannt und soll nicht aus dem Kaffeesatz gewonnen werden. Patent DE 69623762 T2 describes a method for obtaining terpenes, such as cafestolester, diethanol esters and isocafestol esters, by treating the coffee grounds with phosphoric acid and then extracting the terpenes. The disadvantage is that the coffee grounds must be dried before extraction. Extracted oil is called terpene soiling and should not be extracted from the coffee grounds.

US 2010/0287823 A1 offenbart ein Verfahren zur Gewinnung von Biokraftstoffen aus gemahlenem Kaffee. Dabei wird der Kaffee zunächst mit Wasser behandelt und anschliessend zur Gewinnung der Triglyceride mit einem organischen Lösungsmittel wie beispielsweise Methanol, Ethanol, Hexan oder Mischungen aus organischen Lösungsmitteln behandelt. In einer Ausführungsform wird das Wasser von dem gemahlenen Kaffee vor der Extraktion durch beispielsweise Gefriertrocknung oder Destillation getrennt. US 2010/0287823 A1 discloses a method for obtaining biofuels from ground coffee. The coffee is first treated with water and then treated to obtain the triglycerides with an organic solvent such as methanol, ethanol, hexane or mixtures of organic solvents. In one embodiment, the water is separated from the ground coffee prior to extraction by, for example, freeze-drying or distillation.

Der vorliegenden Erfindung liegt die Aufgabe zugrunde ein einfaches, universell anwendbares, effizientes, ökonomisches Verfahren zur Extraktion ölhaltiger Bestandteile aus noch feuchten Kaffeebohnen und/oder feuchten Reststoffen der Kaffeeproduktion bereitzustellen.The present invention has for its object to provide a simple, universally applicable, efficient, economical method for the extraction of oil-containing components from still moist coffee beans and / or moist residues of coffee production.

Die Aufgabe wird gelöst durch ein Verfahren zur feuchten Extraktion von ölhaltigen Bestandteilen aus Kaffeebohnen und/oder Reststoffen der Kaffeeproduktion, wobei die Kaffeebohnen und/oder Reststoffe der Kaffeeproduktion einen Restfeuchtegehalt von 10 bis 95 Ma-%, besonders bevorzugt von 30 bis 85 Ma.-%, ganz besonders bevorzugt von 45 bis 85 Ma.-%, gemessen an der Gesamtmasse der Kaffeebohnen und/oder Reststoffe der Kaffeeproduktion, mit einem Extraktionsmittelgemisch bestehend aus mindestens jeweils einem polaren und einem unpolaren Lösungsmittel extrahiert werden und wobei das Extraktionsmittelgemisch das mindestens eine unpolare Lösungsmittel zu einem Anteil von 45 bis 95 Vol-%, gemessen am Gesamtvolumen des Extraktionsmittels enthält.The object is achieved by a method for wet extraction of oily components from coffee beans and / or residues of coffee production, wherein the coffee beans and / or residues of the coffee production a residual moisture content of 10 to 95% by mass, particularly preferably from 30 to 85 Ma. %, very particularly preferably from 45 to 85% by mass, measured on the total mass of the coffee beans and / or residues of the Coffee production, extracted with an extractant mixture consisting of at least one polar and one nonpolar solvent and wherein the extractant mixture contains the at least one non-polar solvent in a proportion of 45 to 95% by volume, measured on the total volume of the extractant.

Extraktion bezeichnet im Sinne der Erfindung das Herauslösen von mindestens einem Stoff aus dem Extraktionsgut Kaffeebohnen und/oder Reststoffe der Kaffeeproduktion mit einem flüssigen Extraktionsmittelgemisch. Feuchte Extraktion bezeichnet eine Extraktion, bei der noch feuchtes Extraktionsgut, mit einem Restfeuchtegehalt, eingesetzt wird.Extraction referred to in the context of the invention, the extraction of at least one substance from the extraction material coffee beans and / or residues of coffee production with a liquid extractant mixture. Moist extraction refers to an extraction in which still moist extraction material, with a residual moisture content, is used.

Ölhaltige Bestandteile umfasst erfindungsgemäß alle Stoffe, die mit dem erfindungsgemäßen Extraktionsmittelgemisch aus dem Extraktionsgut Kaffeebohnen und/oder Reststoffe der Kaffeeproduktion extrahiert werden können. Bevorzugt handelt es sich bei den ölhaltigen Bestandteilen um Fettsäureester, insbesondere Triglyceride und pflanzliche Fette.According to the invention, oil-containing constituents encompass all substances which can be extracted with the extractant mixture according to the invention from the extraction material coffee beans and / or residues of the coffee production. The oil-containing constituents are preferably fatty acid esters, in particular triglycerides and vegetable fats.

Kaffeebohnen bezeichnet im Sinne der Erfindung alle Arten von Kaffeebohnen, sowohl geröstet als auch ungeröstet sowie Mischungen dieser. Die Kaffeebohnen können vorbehandelt, wie beispielsweise sortiert oder gemahlen sein. Gemahlene, nicht extrahierte/gebrühte Kaffeebohnen werden auch als Kaffeemehl bezeichnet.Coffee beans referred to in the context of the invention, all types of coffee beans, both roasted and unroasted and mixtures of these. The coffee beans may be pretreated, such as sorted or ground. Ground, un-extracted / brewed coffee beans are also referred to as ground coffee.

Reststoffe der Kaffeeproduktion umfassen erfindungsgemäß alle Arten von Rückständen (auch Kaffeereste), sowohl Abfall- und Nebenprodukte aus der Kaffeeindustrie. Dazu zählen beispielsweise Kaffeegrund, Kaffeemehl, Separator- und Dekanterschlämme sowie Mischungen aus diesen. Reststoffe fallen beispielsweise bei der industriellen Löskaffeeproduktion sowie in privaten Haushalten oder der Gastronomie an.Residues of coffee production include according to the invention all types of residues (including coffee residues), both waste and by-products from the coffee industry. These include, for example, coffee grounds, ground coffee, separator and decanter sludge and mixtures thereof. Residuals are, for example, in the industrial Löskaffeeproduktion as well as in private households or catering.

Die industrielle Herstellung von Löskaffee umfasst im Wesentlichen folgende Schritte, wobei die technische Ausführung in Details je nach Firma voneinander abweichen können: Die Bohnen werden geröstet und zu Kaffeemehl gemahlen. Das Kaffeemehl wird anschließend durch heißes Wasser und gegebenenfalls unter Druck mehrfach extrahiert (gebrüht), so dass ein Kaffeeextrakt (auch vulgo Kaffee) und ein Kaffeegrund (gebrühtes Kaffeemehl) entstehen. Der Kaffeeextrakt wird anschließend durch Dekanter und Separatoren von Kaffeegrundrückständen gereinigt, zurückgebliebener Kaffeegrund wird als Separator- und Dekanterschlamm bezeichnet. Kaffeeextraktrückstände werden mittels Bandpressen oder anderer Techniken aus dem Kaffeegrund entfernt und nach Reinigung mittels Dekantern und Separatoren wieder der Produktion zugeführt. Anschließend wird der Kaffeeextrakt konzentriert und gefrier- oder sprühgetrocknet, so dass Löskaffeepulver entsteht. Kaffeegrund, Separator- und Dekanterschlämme werden in der Industrie als Abfall betrachtet und der thermischen Verwertung zugeführt. Vorteilhaft können sie aufgrund ihres hohen Wasser- und Ölgehalts dem erfindungsgemäßen Verfahren zugeführt werden.The industrial production of Löskaffee essentially comprises the following steps, wherein the technical execution may vary in details depending on the company: The beans are roasted and ground into ground coffee. The ground coffee is then repeatedly extracted (scalded) by hot water and optionally under pressure, so that a coffee extract (also known as coffee) and a coffee base (brewed ground coffee) are produced. The coffee extract is then cleaned by decanters and separators of coffee grounds residues, remaining coffee grounds is referred to as separator and decanter sludge. Coffee extract residues are removed by means of belt presses or other techniques from the coffee grounds and returned to production after being cleaned by means of decanters and separators. Subsequently, the coffee extract is concentrated and freeze-dried or spray-dried, so that Löskaffeepulver arises. Coffee grounds, separator and decanter sludge are considered as waste in industry and sent for thermal recycling. Advantageously, they can be supplied to the inventive method due to their high water and oil content.

Kaffeegrund bezeichnet erfindungsgemäß die Überreste des Kaffees, insbesondere des Kaffeepulvers und/oder Kaffeemehls, nachdem dieses beispielsweise einem Brühvorgang unterzogen wurde. Kaffeegrund entsteht unter anderem bei der Trinkkaffeezubereitung aber auch bei der Produktion von löslichem Kaffee als Abfallprodukt.Coffee grounds according to the invention denotes the remnants of the coffee, in particular the coffee powder and / or ground coffee, after this has been subjected to a brewing process, for example. Coffee reason arises among other things with the drinking coffee preparation but also with the production of soluble coffee as a waste product.

Vorteilhaft können auch Mischungen aus Kaffeebohnen und Resten der Kaffeeproduktion eingesetzt werden.Advantageously, mixtures of coffee beans and residues of coffee production can be used.

Restfeuchtegehalt ist erfindungsgemäß der Gehalt an Wasser, der sich in den Kaffeebohnen und/oder den Reststoffen der Kaffeeproduktion befindet.Residual moisture content according to the invention, the content of water, which is located in the coffee beans and / or the residues of coffee production.

Extraktionsmittelgemisch ist eine Mischung aus Lösungsmitteln, die zur Extraktion der ölhaltigen Bestandteile verwendet werden können. Vorteilhaft lösen sich die ölhaltigen Bestandteile zumindest teilweise im Extraktionsmittelgemisch. Nach der Extraktion befinden sich die extrahierten öligen Bestandteile gelöst und/oder ungelöst im Extraktionsmittelgemisch. Das Extraktionsmittelgemisch besteht aus einem polaren und einem unpolaren Lösungsmittel. Lösungsmittel werden nach ihrer Polarität (Hydrophilie) eingeteilt. Polar und unpolar beziehen sich im Sinne der Erfindung auch darauf, welches Lösungsmittel beim Vergleich zweier Lösungsmittel das polarere oder unpolarere Lösungsmittel ist. Aufschluss darüber gibt beispielsweise die Elutrope Reihe.Extractant mixture is a mixture of solvents that can be used to extract the oily components. Advantageously, the oil-containing components at least partially dissolve in the extractant mixture. After extraction, the extracted oily components are dissolved and / or undissolved in the extractant mixture. The extractant mixture consists of a polar and a nonpolar solvent. Solvents are classified according to their polarity (hydrophilicity). Polar and nonpolar in the context of the invention also refer to which solvent is the more polar or non-polar solvent when comparing two solvents. The Elutrope series provides information about this, for example.

Bevorzugt sind das polare und das unpolare Lösungsmittel unbegrenzt miteinander, zu mindestens aber in den angegebenen Volumenanteilen, mischbar. Bevorzugt ist das polare Lösungsmittel mit dem mindestens einem zu extrahierenden ölhaltigen Bestandteil mischbar.The polar and nonpolar solvents are preferably immiscible with each other, but at least in the stated proportions by volume, miscible. Preferably, the polar solvent is miscible with the at least one oil-containing component to be extracted.

Bevorzugt wird als mindestens ein unpolares Lösungsmittel, Benzin, Kerosin, Toluol, ein Alkan mit einer Kettenlänge von 5 bis 25 Kohlenstoffatomen oder eine Mischung aus diesen verwendet. Besonders bevorzugt wird ein Alkan mit einer Kettenlänge von 5 bis 12 Kohlenstoffatomen, ganz besonders bevorzugt ausgewählt aus n-Pentan, iso-Pentan, iso-Hexan, n-Heptan, n-Octan, noch mehr bevorzugt n-Hexan, verwendet.Preference is given to using as at least one nonpolar solvent, gasoline, kerosene, toluene, an alkane having a chain length of 5 to 25 carbon atoms or a mixture of these. Particularly preferred is an alkane having a chain length of 5 to 12 carbon atoms, most preferably selected from n-pentane, iso-pentane, iso-hexane, n-heptane, n-octane, even more preferably n-hexane used.

Alkan bezeichnet erfindungsgemäß gesättigte, acyclische Kohlenwasserstoffe mit der allgemeinen Formel CnH2n+2, wobei n ganzzahlig ist. Das Alkan kann sowohl aus einem linearen Kohlenstoffgerüst, als auch aus deren Isomeren und auch verzweigten Kohlenstoffketten bestehen.-Alkane is according to the invention saturated, acyclic hydrocarbons having the general formula C n H 2n + 2, wherein n is an integer. The alkane can consist of both a linear carbon skeleton, as well as their isomers and branched carbon chains.

Bevorzugt wird als polares Lösungsmittel ein Alkohol mit einer Kettenlänge von einem bis 10 Kohlenstoffatomen, besonders bevorzugt von einem bis 6 Kohlenstoffatomen, ganz besonders bevorzugt ausgewählt aus Methanol, Ethanol, Propanol, Butanol und Hexanol, noch mehr bevorzugt 2-Propanol, verwendet.The polar solvent used is preferably an alcohol having a chain length of from 1 to 10 carbon atoms, more preferably from 1 to 6 carbon atoms, most preferably selected from methanol, ethanol, propanol, butanol and hexanol, more preferably 2-propanol.

Erfindungsgemäß enthält das Extraktionsmittelgemisch das unpolare Lösungsmittel zu einem Anteil von 45 bis 95 Vol-%, besonders bevorzugt von 55 bis 85 Vol-%, ganz besonders bevorzugt von 55 bis 75 Vol-%, noch mehr bevorzugt von 60 Vol-%, gemessen am Gesamtvolumen des Extraktionsmittels.According to the invention, the extractant mixture contains the nonpolar solvent from 45 to 95% by volume, more preferably from 55 to 85% by volume, most preferably from 55 to 75% by volume, even more preferably from 60% by volume, based on the total volume of extractant.

Für die in diesem Patent dargestellte Feuchtextraktion werden Mischungen von mindestens einem polaren und einem unpolaren Lösungsmittel genutzt, meist ein Alkan und ein Alkohol. Geeignete Mischungen für die hier dargestellte Feuchtextraktion sind dabei Mischungen mit einem Alkananteil von mindestens 50 Gew.-%, bevorzugt zwischen 55 und 95 Gew.-% und insbesondere zwischen 55 Gew-% und 85 Gew.%.For the wet extraction fraction shown in this patent, mixtures of at least one polar and one non-polar solvent are used, usually an alkane and an alcohol. Suitable mixtures for the moist extraction shown here are mixtures with an alkane content of at least 50 wt .-%, preferably between 55 and 95 wt .-% and in particular between 55 wt% and 85 wt.%.

Bevorzugt enthält das Extraktionsgemisch das mindestens eine polare Lösungsmittel zu einem Anteil von 5 bis 55 Vol-%, besonders bevorzugt zu 15 bis 45 Vol.-%, ganz besonders bevorzugt zu 25 bis 45 Vol.-%, noch mehr bevorzugt von 40 Vol.-%, gemessen am Gesamtvolumen des Extraktionsmittels.The extraction mixture preferably contains the at least one polar solvent in a proportion of 5 to 55% by volume, more preferably 15 to 45% by volume, very preferably 25 to 45% by volume, even more preferably 40% by volume. -%, measured on the total volume of the extractant.

Bevorzugt enthält das Extraktionsgemisch weitere polare und/oder unpolare Lösungsmittel mit einem Volumenanteil von 0,5 bis 40 Vol-%, besonders bevorzugt von 0,5 bis 35 Vol-%, ganz besonders bevorzugt von 0,5 bis 19 Vol-%, gemessen am Gesamtvolumen des Extraktionsmittelgemisches. Die weiteren polaren und/oder unpolaren Lösungsmittel sind aus den erfindungsgemäßen polaren und unpolaren Lösungsmitteln ausgewählt.The extraction mixture preferably contains further polar and / or non-polar solvents having a volume fraction of from 0.5 to 40% by volume, more preferably from 0.5 to 35% by volume, very particularly preferably from 0.5 to 19% by volume on the total volume of the extractant mixture. The other polar and / or non-polar solvents are selected from the polar and non-polar solvents according to the invention.

Alternativ aber nicht ausschließlich können auch binäre, tertiäre oder höhere Mischungen verschiedener Alkohole wie Methanol, Ethanol, Propanol und Butanol usw. als alkoholische Phase und Mischungen von Pentan, Hexan, Heptan, Benzin oder Kerosin und dergleichen als Alkanphase genutzt werden. Aber auch Mischungen auf der Basis von Aceton und Toluol sind möglich.Alternatively, but not exclusively, binary, tertiary or higher mixtures of different alcohols such as methanol, ethanol, propanol and butanol, etc. can be used as the alcoholic phase and mixtures of pentane, hexane, heptane, gasoline or kerosene and the like as the alkane phase. But also mixtures based on acetone and toluene are possible.

Bei der Einstellung der Mischung sollte darauf geachtet werden, dass der Alkoholanteil sowohl mit Wasser als auch mit der Alkanphase mischbar ist. Ist dies erfüllt, ist es möglich, feuchte Materialien direkt zu extrahieren, ohne eine Trocknung oder nur eine geringe Trocknung vorzunehmen.When adjusting the mixture, care should be taken that the alcohol content is miscible both with water and with the alkane phase. If this is achieved, it is possible to extract moist materials directly, without drying or only a small amount of drying.

Bevorzugt wird das Extraktionsmittelgemisch mit einer Temperatur oberhalb der Umgebungstemperatur aber unterhalb des Siedepunktes des am niedrigsten siedenden Lösungsmittels bzw. des am niedrigsten siedenden Azeotropes des Extraktionsmittelgemisches, eingesetzt wird. Ein Azeotrop ist eine Mischung von mindestens zwei Lösungsmitteln, deren Dampfphase die gleiche Zusammensetzung hat wie die flüssige Phase, wodurch eine destillative Trennung der mindestens zwei Lösungsmittel nicht möglich ist..The extractant mixture is preferably used at a temperature above the ambient temperature but below the boiling point of the lowest-boiling solvent or the lowest-boiling azeotrope of the extractant mixture. An azeotrope is a mixture of at least two solvents whose vapor phase has the same composition as the liquid phase, whereby a distillative separation of the at least two solvents is not possible.

Die Effizienz des Extraktionsprozesses steigt dabei wie alle chemischen und physikalischen Prozesse mit steigender Temperatur. Die maximale Arbeitstemperatur entspricht dabei dem Siedepunkt der flüchtigsten Komponente der Extraktionslösung, welche auch ein Azeotrop verschiedener Komponenten sein kann.The efficiency of the extraction process increases as all chemical and physical processes with increasing temperature. The maximum working temperature corresponds to this Boiling point of the most volatile component of the extraction solution, which may also be an azeotrope of various components.

Vorteilhaft wird die Temperatur auch nur so hoch gewählt, dass die zu extrahierenden ölhaltigen Bestandteile nicht negativ durch die einwirkende Wärme verändert werden.Advantageously, the temperature is chosen only so high that the oil-containing components to be extracted are not negatively changed by the applied heat.

Bevorzugt ist ein warmes Extraktionsmittelgemisch mit einer Temperatur von 35 bis 69°C, ganz besonders bevorzugt von 50 bis 65°C, ganz besonders bevorzugt von 58 bis 63°C. Vorteilhaft liegt die Temperatur nur geringfügig (0 bis 6°C) unterhalb des Siedepunktes von n-Hexan (Siedepunkt: 69°C).Preference is given to a warm extractant mixture having a temperature of from 35 to 69.degree. C., very particularly preferably from 50 to 65.degree. C., very particularly preferably from 58 to 63.degree. Advantageously, the temperature is only slightly (0 to 6 ° C) below the boiling point of n-hexane (boiling point: 69 ° C).

Vorteilhaft wird durch den Einsatz eines warmen Extraktionsmittelgemisches der Extraktionsgrad erhöht, d.h. es kann mit einem Extraktionsmittelgemisch mit erhöhter Temperatur eine größere Menge ölhaltiger Bestandteile entfernt werden als mit dem gleichen Volumen des gleichen Extraktionsmittelgemisches welches lediglich Umgebungstemperatur aufweist.Advantageously, the extraction rate is increased by the use of a warm extractant mixture, i. It can be removed with an extractant mixture with elevated temperature, a larger amount of oily ingredients than with the same volume of the same extractant mixture which has only ambient temperature.

Bevorzugt werden Kaffeebohnen und/oder Reststoffe der Kaffeeproduktion mit einer durchschnittlichen Korngröße von 0,001 bis 10 mm, besonders bevorzugt von 0,01 bis 5 mm, ganz besonders bevorzugt von 0,01 bis 2 mm eingesetzt. In einer besonderen Ausgestaltung der Erfindung weisen die Kaffeebohnen und/oder Reststoffe der Kaffeeproduktion zu mindestens 30 Ma-%, gemessen am Gesamtgewicht der Kaffeebohnen und/oder Reststoffe der Kaffeeproduktion, eine durchschnittliche Korngröße von kleiner gleich 2 mm auf.Preferably coffee beans and / or residues of the coffee production are used with an average particle size of 0.001 to 10 mm, more preferably from 0.01 to 5 mm, most preferably from 0.01 to 2 mm. In a particular embodiment of the invention, the coffee beans and / or residues of coffee production to at least 30% by mass, measured on the total weight of the coffee beans and / or residues of coffee production, an average grain size of less than or equal to 2 mm.

Korngröße bezeichnet im Sinne der Erfindung die durchschnittliche Größenverteilung der Partikel innerhalb eines Gemenges an Kaffeebohnen und/oder Reststoffen der Kaffeeproduktion.Grain size in the context of the invention means the average size distribution of the particles within a batch of coffee beans and / or residues of coffee production.

Für die Effizienz des Prozesses ist es vorteilhaft, wenn das öltragende Material so fein wie möglich ist. Je kleiner die Partikel des öltragenden Materials, desto schneller und effizienter kann das Extraktionsmittel eindringen und das Öl lösen. Ist das Verhältnis von Oberfläche zu Volumen zu klein, dauert das Eindringen des Extraktionsmittels zu lange und auch verbleiben erhebliche Mengen des Extraktionsmittels in dem Material, nachdem die Miscella abgezogen wurde. Miscella bezeichnet ein Stoffgemisch aus einem Extraktions(-gemisch) und mindestens einem extrahierten Öl.For the efficiency of the process, it is advantageous if the oil-bearing material is as fine as possible. The smaller the particles of the oil-bearing material, the faster and more efficiently the extractant can penetrate and dissolve the oil. If the surface to volume ratio is too small, the extractant penetration will take too long and significant amounts of the extractant will remain in the material after the miscella has been withdrawn. Miscella refers to a mixture of an extraction (mixture) and at least one extracted oil.

Alternativ oder in Kombination kann das öltragende Material auch vorher gemahlen werden, um eine optimale Materialgröße zu erhalten. Die maximale Partikelgröße sollte dabei unter 5 mm liegen und besser noch unter 2 mm. Insbesondere sind Partikelgrößen unter 1 mm anzustreben, wobei mindestens 30 Gew.-% des öltragenden Materials eine Partikelgröße kleiner als 2 mm im trockenen Zustand aufweisen sollten.Alternatively or in combination, the oil-bearing material may also be previously ground to obtain an optimum material size. The maximum particle size should be less than 5 mm and better still less than 2 mm. In particular, particle sizes below 1 mm are to be striven for, wherein at least 30% by weight of the oil-carrying material should have a particle size of less than 2 mm in the dry state.

Bevorzugt werden Kaffeebohnen und/oder Reststoffe der Kaffeeproduktion mit einem Gehalt an ölhaltigen Bestandteilen von 5 bis 60 Ma-% in der Trockenmasse (i. Tr.), besonders bevorzugt von 10 bis 45 Ma-% i. Tr., ganz besonders bevorzugt von 15 bis 35 Ma-% i. Tr., gemessen an der Gesamttrockenmasse der Kaffeebohnen und/oder Reststoffe der Kaffeeproduktion, eingesetzt.Preference is given to coffee beans and / or residues of the coffee production with a content of oil-containing constituents of from 5 to 60% by mass in the dry mass (absolute tr.), Particularly preferably from 10 to 45% by mass. Tr., Most preferably from 15 to 35% by mass. Tr., Based on the total solids of the coffee beans and / or residues of coffee production used.

Gesamttrockenmasse bezeichnet erfindungsgemäß die Gesamtmasse der Kaffeebohnen und/oder Reststoffe der Kaffeeproduktion nach dessen vollständiger Trocknung bis zur Massekonstanz.Total dry mass according to the invention denotes the total mass of the coffee beans and / or residues of the coffee production after its complete drying to constant mass.

Vorteilhaft können 50 bis 100 Ma-%, besonders bevorzugt 65 bis 99 Ma-%, ganz besonders bevorzugt 70 bis 99 Ma-% der ölhaltigen Bestandteile, gemessen an der Gesamtmasse der Kaffeebohnen und/oder der Reststoffe der Kaffeeproduktion extrahiert werden.
Bevorzugt werden die ölhaltigen Bestandteile nach der Extraktion von dem Extraktionsmittelgemisch destillativ getrennt.
Die Trennung der extrahierten ölhaltigen Bestandteile von dem Extraktionsmittelgemisch kann beispielsweise über mehrere Stufen erfolgen, wobei zunächst die an leichtesten flüchtige Komponente und dann sukzessive die schwerer flüchtigen Bestandteile abgetrennt werden. Vorteilhaft kann aus zurückgewonnenem Lösungsmittel wieder ein Extraktionsmittelgemisch hergestellt werden.
Durch Destillation der Miscella wird das Öl vom Lösungsmittel getrennt, wie in einem konventionellen Extraktionsprozess auf der Basis von Hexan als Extraktionsmittel. Durch die Destillation wird nicht nur das Öl von der Extraktionslösung getrennt, sondern es können auch die Komponenten des Extraktionsmittels voneinander separiert werden. Werden diese im selben Behälter aufgefangen und kombiniert, kann die Mischung wieder als Extraktionsmittel genutzt werden. Werden die einzelnen Komponenten getrennt, kann im laufenden Betrieb das Extraktionsmittel auf abweichende Eigenschaften des Extraktionsgutes angepasst werden, wenn der Aufbau der Anlage dies zulässt. Durch die unterschiedlichen Bestandteile des Extraktionsmittels haben die einzelnen Komponenten unterschiedliche Tendenz, im entölten Grundmaterial zu verbleiben. Dies führt dazu, dass sich die anteilige Zusammensetzung der Extraktionslösung mit der Zeit verändert und das Verhältnis der Bestandteile den voreingestellten, optimalen Bereich verlässt. Entsprechend ist es nötig, regelmäßig die Zusammensetzung der Extraktionsmischung zu prüfen und gegebenenfalls neu zu justieren. Dies kann beispielsweise über die Bestimmung der Dichte geschehen, aber auch andere Methoden wie Fluoreszenzmessungen sind denkbar. Auch können Fluoreszenzmessungen genutzt werden, um den Ölgehalt in der Miscella zu kontrollieren und zu bestimmen, wann Sättigung erreicht ist und das Solvens erneuert werden muss.
In einer besonderen Ausgestaltung der Erfindung werden zur Extraktion ölhaltiger Bestandteile aus Kaffeebohnen und/oder Reststoffen der Kaffeeproduktion Mischungen von 50 Gew.-% - 95 Gew.-% n-Hexan und 5 Gew.-% bis 50 Gew.-% 2-Propanol genutzt, um ohne Trocknung 70 - 98 Gew.-% des Öls aus Materialien (Kaffeebohnen und/oder Reststoffe der Kaffeeproduktion) mit einem Feuchtigkeitsgehalt zwischen 55 und 75 Gew.-% und einem Ölgehalt zwischen 15 und 35 Gew.-% in der Trockenmasse zu gewinnen.
Besonders zu bevorzugen ist dabei, dass auch das Öl mit der alkoholischen Phase mischbar und idealerweise auch in ihr lösbar ist. Ist dies gegeben, so ist es möglich über 90 % des Öls aus feuchten, ölhaltigem Material zu lösen und mittels Destillation vom Extraktionsmittel zu trennen, wie bei einem herkömmlichen Extraktionsverfahren mit n-Hexan als Solvens.
Der Prozess der Feuchtextraktion kann prinzipiell auf allen Anlagen gefahren werden, welche für die Hexanextraktion ausgelegt sind, wie Perkulations- und kontinuierliche Bandanlagen. Einzig muss die Destillationseinheit in der Lage sein, bei höheren Temperaturen betrieben zu werden, als bei der Nutzung von reinem Hexan, da die Alkohole meist höhere Siedepunkte als Hexan haben. Gegebenenfalls müssen Dichtungen genutzt werden, welche in der Lage sind sowohl Alkanen als auch Alkoholen zu wiederstehen. Auch ist hervorzuheben, dass aus dem Material Farb- und Schwebstoffe in das Extrakt übergehen können, welche normalerweise nicht bei einer reinen Hexanextraktion im Öl zu finden sind. Dies liegt an dem Alkoholanteil, welcher im gewissen Maße den Übergang hydrophiler Substanzen ermöglicht. Um diese aus dem Öl zu entfernen, kann ein weiterer Filterschritt in den Prozess integriert werden, welcher es erlaubt, eventuell vorhandene Schwebstoffe aus dem Öl zu entfernen. Die weitere Aufbereitung des Öls findet nach der Abscheidung vom Lösungsmittel und der Filtration in einer Ölraffiniere statt und ist nicht mehr Teil dieses Verfahrens. Auch kann durch eine Reduktion des Alkoholanteils der Prozess zu einem reineren Öl hin optimiert werden, wenn dadurch die Extraktionseffizienz nicht oder nur vertretbar leidet.
Je nach Material können entsprechend Zentrifugen oder Pressen nachgeschaltet sein, um verbleibende Extraktionslösung vom entölten Rohmaterial zu trennen.
Vorteilhaft werden durch das erfindungsgemäße Verfahren laufende und Anfangsinvestitionskosten gegenüber den vorher genannten konventionellen und nicht konventionellen Extraktionsverfahren deutlich reduziert. Das erfindungsgemäße Verfahren stellt somit ein einfaches und universell anwendbares, effizientes, ökonomisches Verfahren zur Extraktion von Pflanzenölen auf der Basis von Triglyceriden aus noch feuchten Materialien, wie Kaffeebohnen und/oder Reststoffen der Kaffeeproduktion, bereit. Vorteilhaft kann das erfindungsgemäße Verfahren auf allen konventionellen Extraktionsanlagen, wenn nötig mit minimalen Modifikationen, durchgeführt werden.
Überraschenderweise hat sich gezeigt, dass in einem Extraktionsmittelgemisch von polaren und unpolaren Lösungsmitteln mit einem höheren Anteil an unpolarem Lösungsmittel ölhaltige Bestandteile, wie beispielsweise Triglyceride, unabhängig vom Wassergehalt aus Pflanzen, wie Kaffeebohnen und/oder Reststoffen der Kaffeeproduktion, ohne Trocknung in sehr guten Ausbeuten extrahiert werden können.
Nach einer besonderen Ausgestaltung der Erfindung werden die Kaffeebohnen und/oder Reste der Kaffeeproduktion mehrfach mit frischem Extraktionsmittelgemisch extrahiert. Bevorzugt erfolgt die Extraktion ein bis 10 mal, besonders bevorzugt ein bis 7 mal, ganz besonders bevorzugt ein bis 5 mal, noch mehr bevorzugt drei mal. Vorteilhaft wird so der Extraktionsgrad gesteigert, d.h. es wird mehr ölhaltiger Bestandteil aus den Kaffeebohnen und/oder Resten der Kaffeeproduktion erhalten. Die einzelnen Extraktionsmittelgemische, die nach einer mehrfachen Extraktion der Kaffeebohnen und/oder Reste der Kaffeeproduktion mit jeweils frischem Extraktionsmittelgemisch erhalten werden, werden vorteilhaft vereinigt. Aus den vereinigten Extraktionsmittelgemischen werden die ölhaltigen Bestandteile destillativ entfernt.
Das vorliegende Verfahren behandelt im Wesentlichen eine Methode zur Erhöhung der Lösungseffizienz der Extraktion von feuchten Materialien, welche es erstmalig ermöglicht feuchte Materialien ohne vorherige Trocknung Energie- und Kosteneffizient zu extrahieren.
Advantageously, 50 to 100% by mass, more preferably 65 to 99% by mass, most preferably 70 to 99% by mass of the oil-containing constituents, measured on the total mass of the coffee beans and / or the residues of the coffee production can be extracted.
Preferably, the oil-containing components are separated by distillation after extraction from the extractant mixture.
The separation of the extracted oil-containing constituents from the extractant mixture can be carried out, for example, over several stages, wherein first the most volatile component and then successively the less volatile constituents are separated off. Advantageously, an extractant mixture can be prepared from recovered solvent again.
Distillation of the miscella separates the oil from the solvent, as in a conventional extraction process based on hexane as extractant. By the distillation not only the oil is separated from the extraction solution, but it can also be the components of the extractant separated from each other. If these are collected in the same container and combined, the mixture can be used again as an extractant. If the individual components are separated, the extractant can be adapted to different properties of the material to be extracted during operation if the structure of the system permits this. Due to the different constituents of the extractant, the individual components have a different tendency to remain in the de-oiled base material. As a result, the proportionate composition of the extraction solution changes over time and the ratio of the components leaves the preset optimal range. Accordingly, it is necessary to regularly check the composition of the extraction mixture and readjust if necessary. This can be done for example by determining the density, but other methods such as fluorescence measurements are conceivable. Also, fluorescence measurements can be used to increase the oil content in the miscella control and determine when saturation is reached and the solvent must be renewed.
In a particular embodiment of the invention, mixtures of 50% by weight to 95% by weight of n-hexane and 5% by weight to 50% by weight of 2-propanol are used for extracting oily constituents from coffee beans and / or residues of coffee production used to dry without 70 - 98 wt .-% of the oil from materials (coffee beans and / or residues of coffee production) having a moisture content of 55 to 75 wt .-% and an oil content between 15 and 35 wt .-% in dry matter to win.
It is particularly preferable that the oil is also miscible with the alcoholic phase and, ideally, also soluble in it. If this is the case, it is possible to dissolve more than 90% of the oil from moist, oily material and to separate it from the extractant by means of distillation, as in a conventional extraction process with n-hexane as solvent.
In principle, the process of moist extraction can be run on all systems which are designed for hexane extraction, such as percolation and continuous belt systems. Only the distillation unit must be able to operate at higher temperatures than when using pure hexane, since the alcohols usually have higher boiling points than hexane. If necessary, seals must be used which are able to withstand both alkanes and alcohols. It should also be emphasized that colorants and suspended matter can be converted into the extract from the material, which normally can not be found in the oil in a pure hexane extraction. This is due to the alcohol content, which allows the transfer of hydrophilic substances to some extent. To remove these from the oil, another filter step can be integrated into the process, which allows to remove any suspended solids from the oil. The further treatment of the oil takes place after the separation of the solvent and the filtration in an oil refiner and is no longer part of this process. Also can be optimized by a reduction of the alcohol content of the process to a purer oil out, if thereby the extraction efficiency is not or only reasonably suffers.
Depending on the material, centrifuges or presses may be connected downstream in order to separate remaining extraction solution from the deoiled raw material.
Advantageously, current and initial investment costs are significantly reduced by the process according to the invention compared with the previously mentioned conventional and non-conventional extraction processes. The process of the invention thus provides a simple and universally applicable, efficient, economical process for the extraction of vegetable oils based on triglycerides from still moist materials, such as coffee beans and / or coffee production residues. Advantageously, the inventive method on all conventional extraction systems, if necessary with minimal modifications.
Surprisingly, it has been found that in an extractant mixture of polar and nonpolar solvents with a higher proportion of nonpolar solvent oily components such as triglycerides, regardless of the water content of plants such as coffee beans and / or residues of coffee production, extracted without drying in very good yields can be.
According to a particular embodiment of the invention, the coffee beans and / or remains of the coffee production are extracted several times with fresh extractant mixture. Preferably, the extraction is carried out one to 10 times, more preferably one to 7 times, most preferably one to 5 times, even more preferably three times. Advantageously, the degree of extraction is thus increased, ie more oily constituent is obtained from the coffee beans and / or residues of the coffee production. The individual extractant mixtures, which are obtained after a multiple extraction of the coffee beans and / or remnants of the coffee production with each fresh extractant mixture, are advantageously combined. From the combined extractant mixtures, the oily components are removed by distillation.
The present method essentially deals with a method for increasing the solution efficiency of the extraction of moist materials, which for the first time enables the efficient and cost-efficient extraction of moist materials without prior drying.

Anhand der aufgeführten Ausführungsbeispiele soll die Erfindung näher erläutert werden ohne sie auf diese zu beschränken.Based on the listed embodiments, the invention will be explained in more detail without limiting it to these.

Beispiel 1 - Feuchte Extraktion mit industriellem Kaffeegrund Example 1 - Wet extraction with industrial coffee grounds

Für die Extraktion mittels binärer Extraktionslösungen wurde frischer, feuchter Robusta Kaffeegrund aus der industriellen Löskaffeeproduktion mit einem Wassergehalt von 68 % und einem Ölgehalt von 17,3 % in der Trockenmasse verwendet.For extraction by means of binary extraction solutions, fresh, moist Robusta coffee base from the industrial dissolving coffee production with a water content of 68% and an oil content of 17.3% in the dry mass was used.

Portionen von je 27 und 28 g feuchten Kaffeegrund wurden jeweils in einen Filter mit einer Porengröße von 100 µm gegeben und in einem Becherglas platziert. Die Bechergläser wurden jeweils mit 100 ml Extraktionslösung zusammengesetzt aus verschiedenen Mischungen von n-Hexan und 2-Propanol mit Volumenanteilen zwischen 45:55 und 85:15 gefüllt und ein Becherglas mit reinem Hexan. Sowohl die Mischungen als auch das reine Hexan waren auf 60 °C erwärmt. Die Proben wurde 10 min in den Extraktionslösungen belassen und anschließend entnommen. Den Proben wurde eine weitere Minute zum Abtropfen gegeben. Anschließend wurden die gewonnenen Miscellae destilliert und das gewonnene Öl gravimetrisch bestimmt. Der Kaffeegrund wurde ebenfalls getrocknet um die jeweilige Masse der Probe zu bestimmen und somit die maximal mögliche zu gewinnende Ölmenge zu bestimmen. Diese theoretische Ölmenge und die tatsächlich gewonnene Ölmenge wurden anschließend in Verhältnis gesetzt. Mittels Feuchtextraktion konnten zwischen 50 und 95 Ma-% des Öls gewonnen werden, wobei die Ausbeute bei einem n-Hexananteil von 70 und 85 Vol.-% zwischen 90 und 97 % lag. Jenseits dieses optimalen Bereiches fiel die Extraktionseffizienz rapide ab und lag bei reinem n-Hexan (100 Vol.-%) bei 0% Ausbeute.Portions of 27 and 28 g of moist coffee grounds each were placed in a filter with a pore size of 100 microns and placed in a beaker. The beakers were each filled with 100 ml of extraction solution composed of various mixtures of n-hexane and 2-propanol with volume fractions between 45:55 and 85:15 and a beaker of pure hexane. Both the mixtures and the pure hexane were heated to 60 ° C. The samples were left in the extraction solutions for 10 minutes and then removed. The samples were given an extra minute to drain. Subsequently, the obtained Miscellae were distilled and the oil obtained determined gravimetrically. The coffee grounds were also dried to determine the respective mass of the sample and thus to determine the maximum possible amount of oil to be extracted. This theoretical amount of oil and the amount of oil actually recovered were then put into proportion. By means of wet extraction, it was possible to obtain between 50 and 95% by mass of the oil, the yield being between 90 and 97% with an n-hexane content of 70 and 85% by volume. Beyond this optimum range, extraction efficiency dropped rapidly and was at 0% yield for pure n-hexane (100% by volume).

Beispiel 2 - Feuchte Extraktion mit Dekanterschlamm aus der Löskaffeeproduktion Example 2 - Wet extraction with decanter sludge from the Löskaffeeproduktion

Für die Feuchtextraktion wurde frischer, feuchter Dekanterschlamm aus der Löskaffeeprodution mit einem Wassergehalt von 75,4 % und einem Ölgehalt von 14,6 % in der Trockenmasse verwendet. Der Dekanterschlamm entstammte der industriellen Löskaffeeproduktion. Portionen zwischen 42 und 43 g feuchten Dekanterschlamms wurden jeweils in einem Becherglas platziert und in 48 bis 49 g Extraktionslösung bei 60°C dispergiert. Bei den Extraktionslösungen handelte es sich um verschiedene Mischungen von n-Hexan und 2-Propanol mit Volumenanteilen zwischen 45:55 und 70:30. Das Material verblieb für 20 min in den Extraktionslösungen. Die Miscella wurden anschließend filtriert und destilliert und die gewonnene Ölmenge gravimetrisch bestimmt. Mittels Feuchtextraktion konnten zwischen 50 und 99 Ma-% des Öls aus Dekanterschlamm ohne Trocknung gewonnen werden.For the wet extraction, fresh, moist decanter sludge from the Löskaffeeprodution was used with a water content of 75.4% and an oil content of 14.6% in the dry mass. The decanter sludge came from the industrial Löskaffeeproduktion. Portions of between 42 and 43 grams of wet decanter sludge were each placed in a beaker and dispersed in 48 to 49 grams of extraction solution at 60 ° C. The extraction solutions were various mixtures of n-hexane and 2-propanol with volume fractions between 45:55 and 70:30. The material remained in the extraction solutions for 20 min. The miscella were then filtered and distilled and determined the amount of oil obtained gravimetrically. By means of wet extraction, it was possible to obtain between 50 and 99% by mass of the oil from decanter sludge without drying.

Beispiel 3 - Feuchte Extraktion mit industriellem Arabica Kaffeegrund Example 3 - Wet extraction with industrial arabica coffee base

Für die Untersuchung wurde tiefgefrorener industrieller Arabica Kaffeegrund mit 60,4 % Restfeuchtigkeit und einem Ölgehalt von 31,2 % i. Tr. untersucht. Dem Kaffeegrund wurde zum Auftauen für 24 h im Kühlschrank bei 7°C gelagert. Für die Untersuchungen wurde eine 65:35 (n-Hexan:2-Propanol) Extraktionslösung genutzt. 50 g Kaffeegrund wurden in einen Filter gegeben und in einem Becherglas platziert. Die Probe wurde mit 100 ml Extraktionsmittelgemisch, erwärmt auf 60°C, aufgegossen und 15 min ruhen gelassen. Anschließend wurde die Miscella abgezogen und dreimal mit je 30 ml warmen Extraktionsmittelgemisch gespült. Es konnten auf diese Weise 89 % des Öls gewonnen werden, während ein Versuch mit warmen n-Hexan eine Ausbeute von weniger als 1 % erbrachte.Deep-frozen industrial Arabica coffee grounds with 60.4% residual moisture and an oil content of 31.2% i. Tr. examined. The coffee base was stored for thawing for 24 h in the refrigerator at 7 ° C for thawing. For the investigations, a 65:35 (n-hexane: 2-propanol) extraction solution was used. 50 g of coffee grounds were placed in a filter and placed in a beaker. The sample was poured with 100 ml extractant mixture, heated to 60 ° C, and allowed to rest for 15 min. Subsequently, the Miscella was withdrawn and rinsed three times with 30 ml of warm extractant mixture. It could be recovered in this way, 89% of the oil, while a test with warm n-hexane yielded less than 1%.

Claims (9)

  1. Method for the wet extraction of oil-containing components from coffee beans and/or residual products of coffee production, wherein the coffee beans and/or residual products of coffee production, having a residual moisture content from 10 to 95 percent by mass, based on the total mass of the coffee beans and/or residual products of coffee production, are extracted by means of an extracting agent mixture consisting of at least one polar and at least one nonpolar solvent, and wherein the extracting agent mixture contains the at least one nonpolar solvent in a proportion of from 45 to 95 vol.%, based on the total volume of the extracting agent.
  2. Method according to claim 1, characterised in that benzine, kerosene, toluene, an alkane having a chain length of from 5 to 25 carbon atoms, or a mixture thereof, is used as at least one nonpolar solvent.
  3. Method according to either claim 1 or claim 2, characterised in that an alcohol having a chain length of from 1 to 10 carbon atoms is used as at least one polar solvent.
  4. Method according to any of claims 1 to 3, characterised in that the extracting agent mixture contains the at least one polar solvent in a proportion of from 5 to 55 vol.%, based on the total volume of the extracting agent.
  5. Method according to any of claims 1 to 4, characterised in that the extracting agent mixture contains additional polar and/or nonpolar solvents having a volume proportion of from 0.5 to 40 vol.% in total, based on the total volume of the extracting agent mixture.
  6. Method according to any of claims 1 to 5, characterised in that the extracting agent mixture is used at a temperature above ambient temperature but below the boiling point of the solvent of the extracting agent mixture having the lowest boiling point or the azeotrope of the extracting agent mixture having the lowest boiling point.
  7. Method according to any of claims 1 to 6, characterised in that coffee beans and/or residual products of coffee production having an average particle size of from 0.001 to 10 mm are used.
  8. Method according to any of claims 1 to 7, characterised in that coffee beans and/or residual products of coffee production having a content of oil-containing components of from 5 to 60 percent by mass, based on the total dry weight of the coffee beans and/or residual products of coffee production, are used.
  9. Method according to any of claims 1 to 8, characterised in that the oil-containing components are separated by distillation after being extracted by the extracting agent mixture.
EP15816418.6A 2014-12-15 2015-12-15 Method for the extraction of oily components from coffee beans and/or of residual materials of coffee production Not-in-force EP3234082B1 (en)

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PCT/EP2015/079739 WO2016096817A1 (en) 2014-12-15 2015-12-15 Method for the extraction of oily components from coffee beans and/or of residual materials of coffee production

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CN110373244B (en) * 2019-08-22 2021-12-24 宿州市杰牌化学有限公司 Production process for preparing lubricating oil by using coffee residual oil
CN111019759A (en) * 2019-12-30 2020-04-17 云南大学 Method for extracting coffee extract from coffee grounds
KR102463374B1 (en) * 2021-03-24 2022-11-08 한국과학기술연구원 A method of simultaneously extracting a non-polar component and a polar component from a natural product using two or more immiscible solvents, and a natural product extract manufactured by the method
CN113426155A (en) * 2021-06-04 2021-09-24 北京理工大学 Comprehensive utilization process of coffee grounds
CN115769848A (en) * 2022-12-09 2023-03-10 苏州金猫咖啡有限公司 Instant coffee and production method and production device thereof

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US4156031A (en) * 1975-07-07 1979-05-22 General Foods Corporation Stabilization of purified coffee oil
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US5397571A (en) 1993-03-25 1995-03-14 W. R. Grace & Co.-Conn. Co-extraction of azadirachtin and neem oil
EP0693547B1 (en) * 1994-07-23 2001-01-24 Societe Des Produits Nestle S.A. Antioxidant composition and process for the preparation thereof
EP0819385B1 (en) 1996-07-16 2002-09-18 Societe Des Produits Nestle S.A. Process for extracting terpenes from spent coffee grounds
US8591605B2 (en) * 2007-07-26 2013-11-26 Board Of Regents Of The Nevada System Of Higher Education, On Behalf Of The University Of Nevada, Reno Methods, systems, and apparatus for obtaining biofuel from coffee and fuels produced therefrom
US8273248B1 (en) 2010-04-06 2012-09-25 Heliae Development, Llc Extraction of neutral lipids by a two solvent method
US8211308B2 (en) 2010-04-06 2012-07-03 Heliae Development, Llc Extraction of polar lipids by a two solvent method
US20130274490A1 (en) * 2012-04-11 2013-10-17 Jeffrey G. Hippler Extraction of Lipids From Algae

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US20170325474A1 (en) 2017-11-16

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